Lead zirconate titanate (PZT) nanopowders with the composition of Pb(Zr0.52Ti0.48)O3were synthesized by a sol–gel process. The prepared PZT powders were calcinated at 500 °C,600 °C,700 °C and 750 °C for 1 h.Thermal, vibrational and Structural characteristic of PZT powder have been studied ,using thermogravimetric analysis (TGA ), fourier transform infrared (FTIR) spectroscope,and powder x-ray diffraction (XRD).Results showed that single phase perovskite pzt powders were obtained at temperature of 750 °C.By using materials analysis using diffraction (Maud) program the anisotropic microstructural characteristics (crystallite size and microstrain)and lattice parameters at different calcination temperature were determined, using anisotropic no rules approach. Also, from the same program weight fractions of tetragonal and rhombohedral phases in pzt powders at different calcination temperaturewere calculated.